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In this work, polyaniline–nickel–zinc–ferrite nanocomposites were synthesized by the in situ polymerization method by varying the concentrations of Ni0.6Z0.4Fe2O4 nanoparticles in the polyaniline matrix (10, 20, 30, 40, and 50 wt%). The synthesized nanocomposites were subjected to structural characterizations viz., X-ray diffraction, Fourier-transform infrared spectroscopy, and field-emission scanning electron microscopy techniques. Fourier-transform infrared spectroscopy and X-ray diffraction spectral studies reveal the presence of characteristic bands of both polyaniline and Ni0.6Z0.4Fe2O4 nanoparticles and the formation of their composites is confirmed with the interfacial interaction of Ni0.6Z0.4Fe2O4 nanoparticles in the polyaniline systems. The field-emission scanning electron microscopy images of polyaniline–Ni0.6Z0.4Fe2O4 nanocomposites show a symmetric morphological variation of Ni0.6Z0.4Fe2O4 nanoparticles compared to polyaniline. The electrical properties of the prepared samples were studied in the frequency range of 100 Hz–5 MHz at room temperature. The gas-sensing performance of the nanocomposites was studied at room temperature for butane gas. The polyaniline–10 wt% Ni0.6Z0.4Fe2O4 nanocomposite shows maximum sensing response (109%) at room temperature for 5000 ppm of butane gas with a good response of 28 s and recovery time of 31 s. The stability of the prepared sample was tested for 60 days.